QuEChERS-UPLC-MS/MS法同时测定青虾中27种兽药残留

Simultaneous Determination of 27 Veterinary Drug Residues in Freshwater Shrimp by QuEChERS-UPLC-MS/MS

[目的]建立超高效液相色谱-串联质谱(UPLC-MS/MS)同位素内标法同时测定青虾中磺胺类、氟喹诺酮类、四环素类、酰胺醇类4大类27种兽药残留量的检测方法。[方法]青虾样品经86%(V/V)酸化乙腈(3%甲酸)-水溶液(含0.1 mol/L EDTA)提取后,提取液经分散固相萃取法净化,以UPLC-MS/MS测定,内标法定量。[结果]27种兽药在各自线性范围内呈良好的线性关系(R^(2)≥0.99),磺胺类、氟喹诺酮类、酰胺醇类、四环素类的定量限分别为2.0、2.0、1.0、50.0μg/kg,回收率在70.1%~110.0%,相对标准偏差(RSD)在0.2%~9.8%。[结论]该方法前处理简单、准确、对环境友好,适用于青虾中兽药残留的高通量快速检测分析。

[Objective]To establish an ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)with isotope-labelled internal standard method,which was used to determine multiclass veterinary drugs residues simultaneously including sulfonamides,fluoroquinolones,tetracyclines and amphenicols in freshwater shrimp.[Method]The samples were extracted with 86%(V/V)acidified acetonitrile(3%formic acid)-water(containing 0.1 mol/L EDTA),then the extract was purified by dispersive solid phase extraction(DPSE).The samples were determined by UPLC-MS/MS and quantified by internal standard method.[Result]27 kinds of veterinary drugs showed good linear relationship in their respective linear ranges(R^(2)≥0.99).The limits of quantification of sulfonamides,fluoroquinolones,amide alcohols and tetracyclines were 2.0,2.0,1.0,50.0μg/kg,respectively.The recovery rates were 70.1%-110.0%.The relative standard deviations were 0.2%-9.8%.[Conclusion]The method is simple,accurate and environment-friendly,which is suitable for high-throughput rapid detection and analysis of veterinary drug residues in freshwater shrimp.